Process of producing saponified material



,April 14; 1936. R E BURNS 2,037,004 I PROCESS OF PRODUCING' SAPONIFIED MATERIAL Filed Jan. 25, 1955 2 sheets-sheet' 1 /Iaz @Trae-maux April 14, 19.36. R, E, BURNS 2,037,004

PROCESS 'OF PRODUCING SAPON-IFIED MATERIAL Filed Jan. 23,1935 2 Sheets- Sheet 2 636 a 1mg/r4.

@a6 Figui y rrae/wsx 4 :a definite :inclv controlled Water content directieya lift' Patented Api". 14

cuirs stores My invention relates saponiecl motericl, such Zil- PRGESS @F PRQDUGENG SAPGNHWD MTE Ralph Everett Bums,

Novelle REM Los Angeles Colli., assigner o corrmrotiom oil slpolieotioo .lumiere 23, 1935, Serial No. 3&39

'2 @Bulimie to the production, oi es soep, rosin sizeu ariel the like, and the principal object of the invention is to produce such e soponitled materiel of from e, saponifleble met erial suoli os/etu oils, by reaction Witii an aqueous solution of a soponiiving reagent such es caustic sodo, caustic potusli, or the like A further object of the invention is to produce suoli saponied -moterlolin granulated or powdered form.

A further object of the invention is to provide process in which oir is introduced into the sezioni fied material during its course of 'manufacture for the purpose of improving its color, decreesing its speciiic gravity, euri increasing the volume of the finished product.

A further object of tlie 'invention is to provide 3@ means for introducing e modifier, suoli es coloring material, filler, or perfumes, into the suponiiieri materiel during tlieours eci its morzuucture for the purpose of moellfyine the characteristics of the iinel product.

Further objects und eovunteges will loe motie,

evident lierelrieitere My invention is well adopted to the produc tion of granular soup from soup ist@ etici its site plication to such manufacture will oe eiescriioe as well illustrating one use to which the process may be put, Without limiting the invention to suoli e. speciiic use, other use s being obvious to one skilled in the ortto which it pertains.

In the process or producing soep,- which is a seponieo. material, it mix un aqueous solution is. standard; practice to oi a soporiiiviug ollrull,

by a suponifyirig alkali to mea-n any used in soep making.

I Wish to be understood of the alkolies which are at present in practice l prefer to use on aqueous solution of caustic socie, although caustic potasio, sodo esli,

muy be used.

The process oi making soap which is generally practiceoi involves the placing of the tot iii e. large lrettle'in which it is heated and to which the alkali is added, the fait be ing agitated during this und other ullrolies (@i., till-m16) addition to Aproduce on intimate mixture of the alkali with. the fst. After thefat and alkali lieve been thoroughly mixed together in the proper proportions, which is readily determined icy .the

skilled soup maker, the charge is heated und ogi- 5 tatou for o. considerable period until practically all of the tots ore broken up und. the fatty soldo Y thereof ore combined with the ollroli.

Ii granules are to loe mode, the process following the soponicotiou of the fats is es follows. lo 'The suponiiied moterielis teken from the kettle emi mixed with :my desired modier as it is run into what is known-ss u crutclier, which is virtuolly e tenir on wheels holding about 1,900 lbs. of soup. lifter the soup und modier ure thoroughle kvA mixed iu the crutcher, the materiel is mu through e. series of steel rolls, Whici'i are chilled, one. sore-pecl off into flakes; these iielres ore then run through oir driers und from .there into o v hummer mill, which brooks them up into granules 2@ My process lios morir advantages over the present soep melone processes, es will be mode evident hereinafter:

l convenient apparatus for corrying' on the process invented bv meis shown in the occom-a zu ponyine cirovviugs, in which:

Fig; l is o diegrorumotic representation oi on assembly of oiolerent units used to curry on the process. s

Fig* 2 is e 'cross-section through u convenient so form of mixer. t

Fie. 3 is o, section tliroueli the ejector nome oi the invention shovvu in Fis. l. Fig? t is o oleo view purtiolly in section oi the lower portion or' the hesiter ti showing' the there 35 mostet eno burner.,

Figo is e, section drown on ori enlarged soule through the right-liano emi of the thermostat os viewed in Fis. l.,

Fis. 6 is o section showing porting the thermostut.

Fig. 7 is u section ou. uri enlorgecl seule through the left-hund emi oi" tire thermostot es viewed. iii Fig. l

the method-oi suioso l, e, reagent pump 2,

tromy the molo.

sllsit l2 through e variable sneed rieur 2l, tl'ie 5o The oppsretus employed consists of u tot pump pump 2 taking reagent through a pipe 22 from a reagent tank 23 and delivering this reagent through a pipe 24 to the mixer 5.

The variable speed gear 2| and certain other variable speed gears 34 and 94, hereinafter referred to, are shown diagrammatically as consisting of two reverse cone pulleys connected by a belt, the position of which on the pulleys can be iixed in any position by the operator of the plant, thus xing the relative speeds of the two pulleys at a ratio between a lower and a higher limit. 'I'his type of variable speed 'drive is used merely for illustrative purposes since it is well known in 'the arts. Other means by which the operator can regulate the proportional feeding of any material may be substituted therefor if desired.

The exact form of the mixer 5 is not important, that shown in Fig. 2, however, being a convenient form. In the form shown a casing 5I surrounds a central pipe 52 through which the reagent is pumped, the fat from the pipe I5 being delivered to the space around this central pipe 52. The reagent and fat are combined or mixed as they leave the mixer 5 and the mixture so produced is delivered through a pipe 53 to the heater 6.

The vheater 6 consists of an outer shell 6I in which is mounted a pipe coil 62. 'I'he lower end of this pipe coil delivers liquid to a thermostat 63 from which the liquid is delivered through a pipe 64 to the cooler 1. A valve or other control device 69 controls the flow of gas or other fuel from a pipe 66 to a burner 61, the valve 69 having the function of regulating the supply of gas passed to the burner. The thermostat 63 forms an automatic means responsive to changes in temperature of the liquid passing therethrough from the coil 62 for actuating the controlldevice. Adjusting means 68 'may be provided on the thermostat. The hot products of combustionffrom the burner 61 constitute a heating medium for the coil 62 and the amount of heat delivered to this coil is, of course, regulated by the amount of gas which is passed to the burner.

'I'he heater shown is that disclosed in the application of Walter B. Kerrick, Serial No. 495,635,

tiled Nov. 14, 1930, Figs. 4, 5, 6, and 7 being drawf ings copied from that application.

The end o1' the coil 62 communicates with an opening 63| which communicates with an inner pipe 632, the end of which is open as shown in Fig. 5 'and which communicates with an Aouter pipe 633. This outer pipe connects to the pipe 64 so that liquid from the coil 62 i'lows through the pipe 632 into the right-hand end of the pipe 633 and inside this pipe from right to left,` this liquid being finally delivered to the pipe 64. Due to the passage of hot liquid through the pipes 632 and 633 `the pipe 633 expands or contracts and operates a valve 69| forming part of the control device 69 as shown in Fig. 5, being operated through a stem 692 from the pipe 633. 'I'he expansion or contraction of the pipe 633 therefore moves the valve 69| towards or away from a. seat 694 which controls the flow of gasA from the pipe 66, thus regulating the amountof gas delivered to the burner 61. 'I'he adjustingfrmeans 68 shown in Fig. 7 tends'v'fto move the thermostat bodily so that the temperature at which the valve 69| closes may be regulated bythe operator at will. The entire thermostat is mounted on a ring 635 which encircles the shell 6| and is supported on suitable lugs 636.. t

The cooler 1 may be of any'convenient form, that shown consisting of a tank 1I inside which is a cooling coil 12, the inlet end of which is connected'to the pipe 64. Cooling water is delivered to the tank 1| through a pipe 3| from the primary Water water pump 3,'this water being taken through a pipe 32 from a water tank 33. The primary water pump 3 is driven from the shaft I2 through a variable speed gear 34. Excess water and steam are removed from the top of the tank drawing materialthrough a pipe 92 from a tank 93. The pump 9 is' driven from the shaft I2 through a variable speed gear 94|.

Ihe granule fabricator I0 consists of a cylindrical shell I 0| in the top of which is placed a nozzle |02 which is connected to the pipe 14. An exhaust fan' |03 draws air from the top of the shell IOI. The shell 0| has an inclined bottom |04 which delivers material through a chute |05 into a closed vstorage chamber |06. A gas inlet pipe I 01 projects through the side of the shell and connects to a ring |08 having perforations |09 inthe bottom thereof. Means not shown for delivering. dry hot air to the pipe |01 are provided. i

'I'he nozzle I 02 is providedV with a constricted orifice I| I, as shown in Fig. 3. The air pump 4 is shown diagrammatically and in practice should be an air compressor capable of pumping air through a pipe 4I into the inlet end of the coil 12 of the cooler regardless of the pressure that may be maintained therein.

T'he materials in the tanks I4, 23, 33, and 93 are replenished from time to time as they be# come partially used and automatic means for accomplishing this may be provided if desired.

If the saponiiiable material which is used is not liquid at room temperatures, means. not shown, must be provided in the tank I4 for heating it so that it is rendered suilciently liquid to pump readily, and heating means, not shown, may also be supplied to the tanks 23, 33, and 93 is desired.

Suitable valves, not shown, are -providedforcontrolling' the iiow of liquids conveniently, andsuitable gaugesand thermometers, not shown, are provided for indicating conditions within the apparatus.

The method of operation is as follows.

Fat is pumped continuously by the pump I from the tank |4 throughthe pipe I5 into the mixer 5. The speed at which the fat is pumped may be regulated by changing the speed of the motor II.

Reagent Ais pumped continuously from the tank 23 to the mixer 5 through the pipe 24 by the pump 2. The variable speed gear 2| permits the rate at which reagent is added to the fat to be varied within limit-s. The proportion of reagent so added depends, of course, upon the character of the fat used. lIf an aqueous solution of caustic soda is used having a a mixture of equal parts of tallow and cocoanut oil is tobe treated, it will be found that if reagent is supplied at the rate of about forty-ve per fat, good results will should be supplied to produce good saponication without leaving too much excess reagent or excess unsaponied fat is, of course,. readily determinable by any skilled soap m'aker.

Using a coil 62 consisting of about 300 feet of gravity of 30 Baume and' The pumps l and'2,

aosacoa pipe 1/2 inch inside diameter, good results can be obtained if from one-third gallon to one gallon per minute of fat is delivered to the mixer 5.

the variable speed gear 2 l, and the mixer 5, taken collectively, constitute a proportioning device having the function of delivering a mixture of fat and reagent (in proper proportions), to the con s2 of the heater. other means of performing this function will be obvious to one skilled in the art. For example, the' mixture of fat and reagent may be produced in the tank i4, in which case the tank 23, the pump 2,

' the`jvariable speed gear 2i, and the mixer 5 may be dispensed with, the pipe l being connected 'tothe pipe l53. The arrangement shown has, however, certain advantages, among which may be mentioned the automatic mixing in the right proportion and the ease by which tais proportion can be changed by varying the speed of the pump 2 by manipulating the' variable speed gear 2l.

The function of the mixer is to bnng the liat and reagent together and while the mixer 'shownjets thev reagent into vthe oil, and this is a convenient method) of producing an intimate mixture, this is not necessary since the iat and reagent are'tlaoroughly .mixed due to the mild turbulence produced in the coil t2.

The function ot raise the temperature of the mixture of. fat and reagent to a point at which saponicat on is ia cilitated. It will be found that excellent results are obtained if a temperature of from 490 to 500" F. is maintained in the coil or. For reasons which will be hereinafter explained it will be found possible to maintain a pressure of from 150 to 50o pounds per square inch on the liquid leaving the coil di? and this pressure also assists in splitting the iat into free fatty acid and glycerine, the

free fatty acid combining with the reagent toV produce soap. The reaction between the iat and reagent seems to -be facilitated by the velity and mild turbulence produced in the mixed iat and reagent as it flows through the coil e2. This turbulence tends to constantly disperse any un- `comb'ned reagent in the body of the mixture so that it is brought into intimate contact with any particles of unsaponiiied iat, thus promoting the desired saponilcation reaction.

The thermostat in the operation of to insure that the the process. Its iuncton is mixture flowing through the l `pipetd is maintained at a vconstant temperature.

Aany increase in 4this temperature expands the pipe @Si and tends to force the valve tsl toward its seat tigt. This tends to reduce the amount ci fuel gas pass'ng to the burner di and this reduces the volume ci the heating medium; that is, the hot products of combustion, burner 5l up into the space surrounding the coil t2 where it is available to heat the mixture of iat and reagent passing through the coil 62.

The material passing through the pipe Gil is preferably in liquid condition. This-material is cooled in the cooler 1. The function of the cooler l is to reduce the temperature of the mixture containing the sapcn'fied material delivered through the pipe 6e, The temperature of the mixture in the pipe B5, in the case of soap manufacture, may be in the neighborhood ol' 500 to 600 F. This high temperature is desirable to produce a rapid-and eiiicient saponiilcatlon. If the mxture were delivered directly to the interior of the granule Iabricator lo or to the open air while at this high temperature, large volumes of water the heater b is primarily to 63 plays an important partpassing from the mxture is cooled in the cooler 'l before being released into the granule fabricator l0.

The degree of this cooling is regulated by ad- .iusting the amount of water supplied tothe cooler l by the pump 3. This regulationl can be conveniently made by adjusting the speed of the pump 3 by the variable speed gear 34. Due to the fact that the pumps l, 2, and 3 are all driven by the shaft l2, all three pumps act as proportioning pumps. so that the amount of cooling in the cooler 'l' is proportionedto the rate of supply of raw materials and varies directly with any variation inthat rate.

.In the production o soap it is often desired tol add to the soap during manufacture certain substances such as inert producing substances, or the like. It is often desirable to introduce such substances after the temperature of the soap has been lowered somewhat from that at which the reaction is produced. For convenience I call all such substances modiilers. They may aiect either the physical or chemical characteristics of the soap, or both.

llers, coloring, or scent Such modifiers may be lconveniently introduced into the coil 'i2 of the cooler l through the pipe di from the pump 9. Since this pump is also driven from the shaft l2 through the variable speed gear ad, the proportion in which modiiier is introduced can be maintained constant or varied by the operator of the plant.

By introducing the air and/or modiiierprior to or during the passage ci the mixture through thecoil of the cooler, the air or modier is distributed throughout the body of the soap due to turbulence produced by the coil. By introducing the' air or modier before the soap is thoroughly cooled by the cooler 'i and while the soap is still very liquid, the uniformity oi this distribution yis promoted. The air and modifier are,

of course, entrained in the soap as it solidifles due to cooling.

b'libe function of the'granule iabricator i@ is to produce granules of soap. By the term granules l mean particles ci soap which may be about the size of mustard seed, although by a suitable nozzle very :fine soap particles can be produced.

This unction is performed by ejecting the partially cooled soap through the constricted 'orice i i i. In practice the soap is cooled in the cooler l to a temperature in the neighborhood of 240 by allowing the water in the cooler l to boil at atmospheric pressure.

With a plant operating under the conditions previously described, a constricted orifice ill which is 5% in diameter and fi, long axially gives excellent results. The soap leaves the con stricted orice ll l with considerable velocity and at the time it leaves the orifice contains some steam and some air which are intimately distributed through the soap granule and which, due to the lowering of pressure in the orifice ill, expand, producing an exceedingly spongy granule. A considerable portion of the steam escapes from the granule into the hot dry ainowing upwardly through the shell lill to the exhauster i133 from the orifices l09 in the ring ill. The soap granules fall slowly through the shell lill and their external surface is dried by the hot dry air so that the granules wilinot stick together lthe chute |05 into the storage chamber |08.

or pack on the bottom IM but will fall through It a heavy granule is desired, i. e., one that will sink in water, no air is injected into the cooler coil 12 through the pipe 4l, in which event the granules are relatively heavy and tend to sink in water almost immediately dissolving if thrown into water, however, due to their sporigy nature. If considerable air is injected, the granules dissolve on the surface of any body of water upon which they are thrown.

'I'his application is a continuation in part of my application Serial 683,162, led August 1,

I claim as my invention:

l. A process of producing a saponied product containing a modifier directly from a saponiliable material by reaction with a saponifying reagent whichcomprises: causing a properly proportioned mixture of a saponiable material and an aqueous solution of a. saponii'ying reagent to flow through a reaction zone in which said reagent reacts with said saponiable material and a suspension containing a saponiled substance is formed, said mixture being at a sutlicient tem- I perature while in said zone to cause a rapid and eilicient reaction between said material and said containing air bubbles directly from a saponiable material by reaction with a saponifying re agent which comprises: passing a properly proand an aqueous solution of said saponifying reagent through a reaction zone in which the saponifying reagent reacts with the saponilable material to produce a suspension containing a saponifying substance, said mixture being at a suiilciently high temperature while in said reaction zone to produce a rapid and elclent reaction between said material and said reagent, in-

jecting compressed air into said suspension while in a state of turbulence whereby to secure an even distribution of the air therein and subjecting the suspension and the injected compressed air to a cooling zone whereby to entrain the air in the soapas it solidifies.

RALPH EVERE'IT BURNS.

-portioned mixture of said saponiable material 

